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WO2000008226A2 - Systemes d'evaporation sous vide activee par plasma, dont les systemes pour l'evaporation d'un solide, la production d'une decharge d'arc electrique et la mesure de l'ionisation et de l'evaporation - Google Patents

Systemes d'evaporation sous vide activee par plasma, dont les systemes pour l'evaporation d'un solide, la production d'une decharge d'arc electrique et la mesure de l'ionisation et de l'evaporation Download PDF

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Publication number
WO2000008226A2
WO2000008226A2 PCT/US1999/015828 US9915828W WO0008226A2 WO 2000008226 A2 WO2000008226 A2 WO 2000008226A2 US 9915828 W US9915828 W US 9915828W WO 0008226 A2 WO0008226 A2 WO 0008226A2
Authority
WO
WIPO (PCT)
Prior art keywords
evaporating
crucible
melting
vapor
electrode
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1999/015828
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English (en)
Other versions
WO2000008226A3 (fr
Inventor
George Plester
Horst Ehrich
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Coca Cola Co
Original Assignee
Coca Cola Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Coca Cola Co filed Critical Coca Cola Co
Priority to AU49906/99A priority Critical patent/AU4990699A/en
Priority to IL14081199A priority patent/IL140811A0/xx
Priority to CA002338352A priority patent/CA2338352A1/fr
Priority to JP2000563847A priority patent/JP2002522637A/ja
Priority to BR9912722-9A priority patent/BR9912722A/pt
Priority to KR1020017000786A priority patent/KR20010083127A/ko
Priority to EP99933968A priority patent/EP1109944A2/fr
Publication of WO2000008226A2 publication Critical patent/WO2000008226A2/fr
Publication of WO2000008226A3 publication Critical patent/WO2000008226A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/243—Crucibles for source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/246—Replenishment of source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation

Definitions

  • This invention generally relates to vacuum vapor deposition coating of substrates and methods and systems involved in vacuum vapor deposition. More particularly, this invention relates to the production of a highly-active and energized plasma-enhanced vapor from a solid source, such as silicon, and to the application of the plasma within a continuously- operating high-speed coating system.
  • the plasma-enhanced vapor may be used for deposition onto plastic articles, particularly for depositing a glass-like coating onto plastic bottles.
  • the coating provides an enhanced gas-barrier and better adhesion compared with prior art coatings, and is suitable for pressurized containers, whose surface flexes and stretches, and whose internal pressure acts against an external coating.
  • the primary component of the vapor is produced by evaporating, in an evaporative source, one or more solids and the deposition of the coating may be applied in conjunction with a reactive gas, or gases, to provide desired coating clarity or colorization. Further, it may be produced by using more than one evaporation source and solids of different boiling points.
  • plastic articles have experienced a growth, because of the properties of these articles such as low-cost, light weight, flexibility, resistance to breakage, and ease of manufacture and shaping.
  • plastics also have the disadvantage of relatively low abrasion-resistance and poor barrier properties against the permeation of vapors such as water, oxygen, and carbon dioxide.
  • limitations in barrier properties have limited the use of plastics. For example, in the case of beverage bottles, inadequate barrier properties have restricted the use of smaller bottles required in some markets. Solutions to this problem, including the use of high-barrier plastics and coatings of various types, have been either uneconomical or have provided inadequate barrier-improvement or add expense to the known recycling processes.
  • the basic anodic system as described by the prior art, has the following disadvantages: a) The crucibles evaporative material content, such as silicon, cannot be replenished continuously when this evaporative material is in powder or pellet/chip form. b) The quantity of vapor evolved from the crucible depends partly on the degree of filling of the crucible with evaporative material. Since the degree of crucible-filling is a variable which constantly changes, this could present a control problem. c) The distribution, at various angular displacements, of the quantity of vapor evolved from the crucible, also depends partly on the degree of filling of the crucible with evaporative material.
  • crucibles for holding silicon are normally constructed of carbon, which is eroded and vaporized by the anodic arc and the carbon vapor is free to form a contaminant in the desired silicon or silicon dioxide coating.
  • the said crucible lip erosion further affects the quantity of vapor evolved and the distribution of this vapor at various angular displacements around the crucible.
  • the anodic arc represents a second and uncontrolled source of heating. This second source of heating partly affects the quantity of vapor evolved, irrespective of any control device for the crucible's independent heating system. This makes process control of evaporation rate difficult, whilst evaporation rate is an important parameter.
  • the quality of a coating on plastic articles is dependent on the control of the degree of ionization and thus on the energy-level of the plasma.
  • a suitably high-energy plasma enables the substrate surface to be cleared of dirt and inert molecules, promoting coating adhesion and coating purity, and further enables coating particles to become embedded in the substrate or to react with the substrate, additionally promoting adhesion.
  • High-energy plasma also promotes the chemical reaction of coating particles with each other, thus forming a dense matrix on the substrate surface, which further enhances adhesion and barrier properties.
  • high-energy plasma induces coating particles to be deposited in a flat, dense physical structure due to the impingement of high-energy collisions, enhancing coating continuity and denseness.
  • over-energized plasma may overheat the substrate, or cause excessive decomposition or degassing from the substrate, or damage the coating.
  • the evolution of gases from the substrate surface during its degassing mixes with the coating particles and reduces coating quality. It is thus important to measure and control plasma energy and degree of ionization. Prior art does not teach how this can be achieved.
  • barrier coating of plastic bottles for carbonated beverages An example of the need for controlled use of high-energy plasma is presented by barrier coating of plastic bottles for carbonated beverages.
  • a barrier coating on a plastic bottle for carbonated beverages must desirably be able to flex, stretch, have adhesion capable of withstanding the pressure migration of the carbon dioxide from the inside of the bottle, and be robust and abrasion resistant in use. It is also desirably dense, preferably amorphous and continuous over the bottle surface.
  • a system and method for continuously melting and evaporating a solid material for use in a vapor deposition coating system a vapor deposition coating system including said continuous melting and evaporating system, a vapor deposition coating system including an electric arc discharge system which switches polarity between electrodes during operation, a vapor deposition coating system comprising an electric arc discharge system including an electrode with combined anodic and cathodic parts for ionization, a continuously fed electrode for producing an electric arc discharge and a coating vapor, a system for measuring the rate of evaporation from an evaporator and the degree of ionization in a vapor deposition coating system, and a self-cleaning vapor deposition coating system.
  • the system of this invention for continuously melting and evaporating a solid material comprises a melting crucible for receiving and melting a solid material to form molten material and an evaporating crucible for evaporating the molten material.
  • the evaporating crucible is connected to the melting crucible in flow communication with the melting crucible for receiving the molten material from the melting crucible and releasing vapor through an opening in the evaporating crucible as the molten material evaporates.
  • This arrangement allows for additional evaporative solid material to be continuously added to the melting crucible without interfering with evaporation of the molten solid in the evaporating crucible.
  • solid evaporative material can be continuously added to the evaporator during operation of the evaporator so that a coating system incorporating this melting and evaporating system can continue uninterrupted for an extended period.
  • the evaporating crucible is separate from the melting crucible, the melting crucible and the evaporating crucible can be heated separately and maintained at different temperatures and the evaporating crucible can be made much smaller than the melting crucible.
  • the evaporating crucible and the melting crucible can be arranged so that the level of molten evaporative material in the evaporating crucible remains substantially constant to provide constant and well directed coating vapor.
  • the corresponding method of this invention for continuously melting and evaporating a solid material therefore comprises the steps of melting the solid material in a melting crucible to form molten material, flowing the molten material from the melting crucible into an evaporating crucible connected to the melting crucible, evaporating the molten material in the evaporating crucible to form a vapor, and releasing the vapor from the evaporating crucible.
  • This system and method of the present invention desirably includes continuously and automatically feeding the solid evaporative material into the melting crucible as the molten material evaporates so as to maintain the molten material in the evaporating crucible at a substantially constant level during evaporation of the molten material.
  • this continuous melting and evaporating system include an arrangement wherein the melting crucible and evaporating crucible are arranged so that the melting crucible and the evaporating crucible hold molten material at the same hydraulic level, an arrangement wherein the evaporating crucible draws the molten evaporative solid from the melting crucible via capillary action, and an arrangement wherein the evaporating crucible draws the molten evaporative material from the melting crucible via thermal syphonic force.
  • inventions include an arrangement wherein a pivoting melting crucible melts solid evaporative material and periodically pours molten evaporative material into an evaporation chamber and an arrangement wherein an electrically heated element melts and evaporates solid evaporative material in a melting crucible.
  • Such embodiments do not require energy from an electric arc discharge for evaporation of the solid material and are simple, relatively inexpensive, and resistant to heat damage.
  • the foregoing system for continuously melting and evaporating a solid evaporative material is particularly useful in a vacuum vapor deposition coating system wherein the continuous melting and evaporating system is disposed within a vacuum cell capable of maintaining a vacuum within the vacuum cell.
  • the vapor deposition coating system and method of the present invention involving switching polarity between electrodes includes forming a vacuum within a vacuum cell, supplying a coating vapor in the vacuum cell, passing the coating vapor through a gap between a first electrode disposed in the vacuum cell and a second electrode disposed in the vacuum cell, supplying electric power to the first and second electrodes so that the first and second electrodes become oppositely charged and create an electric arc discharge between the first and second electrodes, and switching polarity between the first and second electrodes while the electric power is supplied to the first and second electrodes.
  • the switch is desirably operated automatically and repeatedly switches the polarity between the first and second electrodes and the electric power supply is a DC power supply.
  • each electrode By switching the polarity between the first and second electrodes, each electrode alternates between anodic and cathodic function, so that coating vapor, which deposits on the first and second electrodes when the electrodes are in the anodic function, is evaporated when the electrodes are in the cathodic function.
  • the coating vapor when non-electrically conductive, can disrupt the operation of an electrode in a vapor deposition coating system.
  • the first and second electrodes remain substantially free of deposited coating.
  • a vacuum is formed within a vacuum cell, coating vapor is supplied in the vacuum cell, the coating vapor is passed adjacent an electric arc discharge apparatus, and electric power is supplied to the electric arc discharge apparatus so that a cathode portion of the electric arc discharge apparatus becomes negatively charged and an anodic hood, at least partially covering the cathode becomes positively charged, so that an electric arc discharge is created between the cathode and the anodic hood.
  • the electric arc discharge apparatus includes an electrically insulating material connecting the cathode to the anodic hood, and the cathode and the anodic hood are arranged to form an ionization chamber with the anodic hood having a plasma discharge opening.
  • an electric arc discharge is created between the cathode and the anodic hood in the ionization chamber, the cathode emits electrons and ionizes the coating vapor disposed in the vacuum cell by the source of coating vapor, the cathode vaporizes and forms an ionized cathode vapor within the ionization chamber and the ionized cathode vapor is emitted from the discharge opening of the anodic hood and mixes with the coating vapor from the evaporation source and the reactive gas, if any, in the vacuum cell to form a coating plasma.
  • the foregoing method and system are relatively simple and economical for producing a plasma enhanced coating vapor in a vapor deposition coating system.
  • the continuously fed electrode of this invention comprises a plurality of electrode members which vaporize when connected electrically to provide an electric arc discharge, a housing defining a loading chamber for receiving the electrode members in series and including an electrically insulating sleeve, and an electrode member feeder for continuously feeding the plurality of electrode members, in series, through the insulating sleeve in the housing to an electric arc discharge position so that one of the plurality of electrode members is being fed to the electric arc discharge position at a time.
  • This system enables continuous replenishment of the electrodes evaporative material and enables the use of rapidly eroding materials at the cathode of a high energy plasma coating system, enables materials produced by the vaporization of the electrode members to be inco ⁇ orated as dopants in a vapor deposition coating system, and enables substantially uninterrupted production of ionized vapor in an electric arc discharge vapor deposition coating system.
  • the continuously fed electrode functions as a cathode in an electric arc discharge apparatus.
  • the electrode members are desirably elongate rods or cylinders and are automatically fed from a magazine into the loading housing so that the electrode member feeder can continuously feed the plurality of electrode members, in series, to the electric arc discharge position.
  • the continuously fed electrode includes a cooling system for cooling the one electrode member, which is in the electric arc discharge position.
  • the present invention also encompasses an electric arc discharge apparatus comprising the continuously fed electrode described above, an anode, and an electric power supply for supplying electric power to the one electrode member and the anode.
  • the electric power is supplied so that the one electrode member and the anode become oppositely charged with the one electrode having a cathodic charge and the anode having an anodic charge.
  • the present invention encompasses electric arc discharge apparatus comprising the continuously fed electrode described above and an electric power supply.
  • the continuously fed electrode includes a hood for at least partially covering the one electrode member in the electric arc discharge position.
  • An electrically insulating material insulates the one electrode member in the electric arc discharge position from the hood and the hood is arranged to form an ionization chamber into which the electrode members are fed from the housing.
  • the present invention also encompasses a vapor deposition coating system comprising the continuously fed electrode described above and a vacuum cell in which the continuously fed electrode is disposed.
  • This vapor deposition coating system also includes a source of coating vapor disposed in the vacuum cell, a second electrode disposed in the vacuum cell, and an electric power supply for supplying electric power to the one electrode member and the second electrode so that the one electrode member and the second electrode become oppositely charged, create an electric arc discharge and ionize the coating vapor.
  • this vapor deposition coating system further includes an evacuation cell for feeding electrode members into the vacuum cell while the vacuum cell maintains a vacuum.
  • the evacuation cell is capable of receiving electrode members from outside the vacuum cell, evacuating air from the evacuation cell, and feeding the electrode members into the vacuum cell under vacuum without disrupting the vacuum within the vacuum cell.
  • the present invention further encompasses an apparatus for measuring the rate of evaporation from evaporator and the degree of ionization in a vapor deposition coating system comprising two electrical circuits connected to a wire.
  • the first electrical circuit includes a wire, an ammeter connected to the wire for measuring electric current through the wire and a variable DC-power source.
  • a current flows from the said DC-power source, through the ammeter and through the ionized gas to the walls of the ionized gas enclosure or vacuum cell and to ground.
  • the current flow measured by the ammeter, bears a relationship to the degree of ionization in the ionized gas and increases as the degree of ionization increases.
  • the second electrical circuit includes the said wire, a DC or AC supply and a switch.
  • the apparatus desirably includes a timer for controlling the opening and closing of the switch. Particles from the ionized gas deposit on the said wire when the wire is cold and the electrical resistance of theses particles reduces the current flow in the first electrical circuit.
  • a current flows within the second electrical circuit and heats up the said wire, thus causing the deposited particles to re-evaporate, which prevents these particles from insulating the wire and affecting the electrical current flow.
  • the electrical current flow measured in the first electrical circuit therefore retains a constant relationship to the degree of ionization, so long as the wire is heated.
  • the measurement of degree of ionization which this relationship provides, can be used to control the degree of ionization, by means of adjusting the current flow from the power supply to the electric arc by conventional means.
  • the wire cools and particles from the ionized gas begin to deposit on the wire.
  • the electrical resistance of these particles reduces the current flow in the first electrical circuit and the rate of reduction bears a relationship to the rate of deposition of particles, which in turn bears a relationship to the rate of production of coating particles by the evaporator and electric arc means.
  • the rate of evaporation can thus be controlled by adjusting the current flow from the power supply to the evaporator by conventional means.
  • the vapor deposition system itself is as described above and includes an enclosure or cell, which must normally be maintained under vacuum, and a source of ionized coating vapor which is disposed within the said cell.
  • the self-cleaning means includes one electrode, or a plurality of electrodes, disposed within the cell.
  • the electrodes are connected to a power supply and are arranged so that the entire gas space within the cell can be subjected to an ionizing discharge. Suitable forms of power supply include HF, RF and DC.
  • the volatile components of the deposits within the interior of the cell and its internal parts are removed by supplying sufficient ionizing power to the electrode or electrodes disposed in the vacuum cell to ionize gas in the vacuum cell so that the ionized gas removes the deposited coating vapor. This could be done during the operation of the coating system or while the coating system is inoperative.
  • Fig. 1 is a schematic diagram of an evaporator system, made according to an embodiment of this invention, including a continuously-fed melting crucible connected to an evaporating crucible.
  • Figs. 1A, IB, 1C, ID and IE are schematic diagrams of optional arrangements of a continuously-fed dual crucible system, according particular embodiments of the present invention.
  • Fig. 2 is a schematic diagram of an evaporator system, made according to an embodiment of this invention, wherein vapor is energized to a plasma state by means of the arc generated by a pair of DC electrodes, whose relative polarity periodically alternates.
  • Fig. 2A is a schematic diagram of an evaporator system similar to that shown in Fig. 2, except with two pairs of electrodes whose relative polarity periodically alternates.
  • Fig. 3 is a schematic diagram of an evaporator system, made according to an embodiment of this invention, wherein vapor is energized to a plasma state by means of the discharge from a cathode/anode combination.
  • Fig. 4 is a side elevation view of a continuously fed electrode made according to an embodiment of this invention.
  • Fig. 4A is a sectional end view of the electrode illustrated in Fig. 4.
  • Fig. 4B is a schematic diagram of an electrode member feeder for the continuously fed electrode illustrated in Fig. 4.
  • Fig. 5 is a schematic diagram of a system for measuring the rate of evaporation and degree of ionization within a vacuum vapor deposition coating system, in accordance with an embodiment of this invention.
  • Fig. 5A is an example graph of current versus voltage when measuring degree of ionization with the electric circuit illustrated in Fig. 5.
  • Fig. 5B is a schematic diagram illustrating an alternative system for measuring the rate of evaporation and degree of ionization within a vacuum vapor deposition coating system, in accordance with an embodiment of this invention.
  • Fig. 6 is a schematic diagram of a vacuum chamber with several DC-discharge probes (or alternatively RF or HF antennas) mounted within it, enabling discharge within the interior of the vacuum chamber, in accordance with an embodiment of this invention.
  • this invention encompasses vacuum vapor deposition systems and methods, and systems and methods for use in vacuum vapor deposition onto substrates.
  • the following includes a detailed description of embodiments of this invention including evaporator systems and methods, electric arc discharge systems and methods with polarity switching electrodes, electric arc discharge systems and methods with a combination cathodic/anodic electrode, electric arc discharge systems and i methods with a continuously fed electrode, a system and method for measuring rate of evaporation and degree of ionization in a vapor deposition coating system, and a self-cleaning vacuum vapor deposition coating system.
  • like reference numerals are used to refer to like parts throughout the Figures.
  • Fig. 1 shows an evaporator system suitable for a solid, such as silicon, and principally comprising a melting crucible 1 , a molten evaporative material 2, a short conduit 3, and an evaporating crucible 4 connected in fluid flow communication to the melting crucible by the short conduit, the evaporating crucible being in the form of a straight-through, relatively narrow bore pipe.
  • the melting crucible 1 and the evaporating crucible are side-by-side.
  • the melting crucible 1 is heated by a melting crucible heater 5, which is a suitable, conventional device, and normally consists either of a radiant heater, or a contact heater, or a resistance heater.
  • a radiant heater complete with an external heat insulating mantle is an effective solution.
  • the melting crucible heater 5 is provided with an adjustable AC or DC power- supply 6 and this power supply incorporates the necessary conventional means for controlling the energy output of the melting crucible heater 5 so as to provide temperature control.
  • the solid evaporative material 7 to be melted is fed through an opening in the melting crucible 1 in the form of powder or chips or pellets or the like by means of a feeder such as a chute 8.
  • a feeder such as a chute 8.
  • Suitable solid evaporative materials for vacuum vapor deposition coating include silicon and are listed in PCT International Application PCT/US98/05923, already incorporated herein by reference.
  • the design of the feed-system, connected to chute 8 is not shown, and will depend on the material and its form, and employ conventional material feed means.
  • the material in the case when silicon is used as the solid evaporative material, the material would preferably be in form of pellets, and the feed system would include a silo or bin to hold the said pellets, and a valving system at base of the silo/bin to enable a controlled amount of pellets to flow down chute 8 whenever the melting crucible 1 requires material make-up. Said material make-up is necessary whenever the level 9 of molten evaporative material in the melting crucible 1 drops by a predetermined amount.
  • the level 9 of molten evaporative material can be monitored by a level-monitor 10, using conventional non-contact methods such as X-rays, ultrasound, or by weighing the melting crucible 1 , together with any components rigidly attached to it.
  • the molten evaporative material 2 flows from the melting crucible 1 through the conduit 3 to the evaporating crucible 4.
  • the evaporating crucible 4 is heated by the evaporating crucible heater 11 and a separate, adjustable, evaporating crucible power supply 12, employing similar conventional means as already described for the heating of melting crucible 1.
  • the evaporating crucible 4 is heated to a temperature suitable for evaporating the molten evaporative material 2 in the evaporating crucible and the coating vapor produced is released from the evaporating crucible through an opening 13 in the top of the evaporating crucible.
  • the power supply 12 for the evaporating crucible 4 is independently controlled from the power supply 5 for the melting crucible 1 so that the temperature of the melting crucible, which is desirable larger than the evaporating crucible, can be maintained at a lower level than the temperature of the evaporating crucible.
  • the hydraulic level 9 of material 2 in the melting crucible 1 equates to the hydraulic level in the evaporating crucible 4 due to natural hydraulic forces.
  • this automatically maintains a substantially constant and correct level in the evaporating crucible 4 as the molten evaporative material evaporates, and thus the conditions for constant vapor evolution rate and constant particle distribution from the evaporating crucible are achieved.
  • the rate of evaporation from the evaporating crucible 4 is controlled by regulating the energy input to the evaporating crucible power supply 12, using conventional heater power regulation means.
  • the rate of evaporation from the evaporating crucible 4 is adjusted to give the desired rate for the coating process by means described hereinafter.
  • the melting crucible 1 is provided with a lid 15 to reduce migration of vapor. Excessive vapor in this melting crucible 1 can adversely affect the material feed system to chute 8 and the heaters 5 and 11. Ideally, the melting crucible 1 should be maintained at a temperature which is sufficient to melt the evaporative material 2 while producing minimal vapor. Control of the temperature of the evaporative material 2 in the melting crucible 1 is through the energy input from power supply 6 and this energy input is regulated by conventional means.
  • the energy regulator can be controlled according to the rate of in-flow of pellets 7, which in-flow will normally be constant, or, optionally, according to the temperature measurement 16 of the evaporative material 2 by conventional non-contact means such as IR-measurement.
  • temperature measurement 16 can be by an electric resistance thermometer or a bi-metallic thermocouple embedded in the walls of the melting crucible 1.
  • a heat shield 17 constructed of reflective material of suitable heat and corrosion resistance, such as stainless steel, covers the melting crucible 1 and the connecting conduit 3.
  • the system illustrated in Fig. 1 is particularly advantageous with respect to avoiding heat damage of coated articles, since the only part able to radiate heat directly onto the coated articles is the evaporating crucible 4, whose dimensions are small because the evaporating crucible has little capacity due to its continuous feed.
  • the melting crucible 1 can be linked to more than one evaporating crucible 4 by means of multiple conduits 3 where this is needed by a specific system. Such an arrangement reduces the cost and/or complication of multiple solid feed systems to the chute 8.
  • Construction materials for the evaporator system described will depend on the material 2 to be evaporated. Generally, suitable construction materials for the evaporator system can withstand the high temperature necessary to melt and evaporate the solid evaporative material 2 without deteriorating or melting and must be inert to the evaporative material 2.
  • system components 1, 3 and 4 are preferably constructed of a heat conductive grade of carbon.
  • Fig. 1A, IB and 1C show versions of the system illustrated in Fig. 1 not requiring the short connecting conduit 3, since this feature can lead to leaks with molten evaporative materials 2 of certain substances.
  • a melting crucible la is heated by a melting crucible heater 5a and an adjustable power-supply 6a.
  • a tubular evaporating crucible 4a is mounted within the melting crucible la so that the melting crucible holds the molten material 2 at a first level and the evaporating crucible holds the molten material at a second level which is above the first level and the evaporating crucible, at least partially submerged in the molten material, draws the molten material from the melting crucible, through the evaporating crucible, to a vapor releasing opening 13a via capillary action.
  • the top of the tubular evaporating crucible 4a extends through an opening in the melting crucible lid 15a and is heated by the evaporating crucible heater 11a and the associated adjustable power-supply 12a, and thus the temperature of the molten evaporative material is brought from melting temperature level to evaporation temperature level.
  • An overflow cavity 18 is positioned to allow excess molten material 2 to drip back into the melting crucible la.
  • This overflow cavity 18 enables the outside of the top of the tubular evaporating crucible 4a to remain essentially free of molten evaporative material 2 and thus the top of tubular evaporating crucible 4a may be heated by conventional radiant or resistance heating.
  • a heat shield 17a is positioned above the melting crucible la for the same purpose, and with same basic construction, as already described with regard to Fig. 1. Vapor is emitted from the release opening 13a at the top of the tubular evaporating crucible 4a in same manner as described under Fig. 1.
  • a melting crucible lb has a well 19 extending below the bottom of the melting crucible and an adjustable power supply 6b.
  • the foot of the tubular evaporating crucible 4b fits tightly into the well 19 and can be fed with molten evaporative material 2 from the melting crucible lb by a small channel 20 and the upper portion of the evaporating crucible extends out of the melting crucible through an opening in the lid 15b of the melting crucible.
  • the tubular evaporating crucible 4b is mounted within the melting crucible lb so that the melting crucible lb holds the molten material 2 at a first level and the evaporating crucible holds the molten material at a second level which is above the first level and the evaporating crucible, at least partially submerged in the molten material, draws the molten material from the melting crucible, through the evaporating crucible, to a vapor releasing opening 13a via thermal syphonic forces.
  • the well 19 is externally heated by the evaporating crucible heater l ib and associated adjustable power supply 12b to evaporating temperature, as is the upper portion of the evaporating crucible 4b proximate a vapor releasing opening 13b.
  • molten evaporative material 2 rises up the tubular evaporating crucible 4b and excess molten evaporative material 2 continuously overflows back down to the melting crucible lb via a series of cavities 18a.
  • a heat shield 17b is provided for the same pu ⁇ ose and with same basic construction as already described above.
  • Vapor is emitted from the vapor release opening 13b in the top of the tubular evaporating crucible 4b in the same manner as already described under Fig. 1.
  • Control of the temperature of the evaporative material 2 and of the evaporative material level 9 are also as described under Fig. 1.
  • a tubular evaporating crucible 4c is an integral part of a melting crucible lc and its spout-like extension l'c. This arrangement can be beneficial where it is difficult to seal vapor evolution from molten evaporative material 2 through component joints, since such joints are completely avoided in Fig. IC.
  • the flow of pellets 7 now flows into the spout-like extension l'c so as to the maintain the level 9 of the evaporative material substantially constant.
  • the melting crucible lc inco ⁇ orates a loose- baffle l"c which is introduced through the opening of spout-like extension l'c and this loose-baffle l"c prevents unmolten pellets 7 from flowing to the tubular evaporating crucible 4c.
  • the evaporator system in Fig. IC functions similarly to the systems already described with regard to Figs. 1, 1A, and IB, and inco ⁇ orates a melting crucible heater 5c, an evaporating crucible heater 1 lc, associated adjustable power supplies 6c and 12c, and a heat shield 17c.
  • Fig. ID shows a method of melting the evaporative material 2 in a batchwise-operating melting crucible Id which is heated, in the manner already described, by crucible heater 5d and power supply 6d.
  • the melting crucible Id receives a fixed batch of solid pellets 7 via chute 8d when in its upright position (shown in solid line).
  • the melting crucible Id can be tilted to a pouring position (shown in chain-clothed line) and in this position releases a required amount of molten material 2, which flows down conduit 3 to evaporating crucible 4d.
  • the released amount of material 2 is controlled by a level-monitor 10a such as to maintain an hydraulic level 9.
  • melting crucible Id As material 2 is evaporated in evaporating crucible 4d, level 9d falls and the filling operation, by means of tilting melting crucible Id, is repeated.
  • Melting crucible Id can be fitted with a pouring spout I'd and a pouring sieve l "d to avoid drips and to avoid passage of relatively large solid pieces of material 2 to the evaporating crucible 4d.
  • the evaporating crucible 4d is heated by the evaporating crucible power supply 12d, using conventional heater power regulation means.
  • the tilting of melting crucible Id is by conventional means (not shown).
  • Fig. IE shows a means of avoiding the need for an evaporating crucible, particularly where the evaporative material 2 is nearly electrically non-conducting in the cold solid state, but gradually increases its conductivity as the solid is heated and further increases its conductivity in the molten state as in the case of silicon.
  • Solid pellets 7 are fed to melting crucible le via chute 8e so as to maintain an approximate pellet level 9e.
  • An electrical circuit is formed between an adjustable power supply 6e, via a switch 81 and via an electrically conductive evaporative element or rod 4e, which is in contact with the base of crucible le.
  • the rod 4e is heated by the current in the said electrical circuit and can therefore melt the solid pellets 7 of material 2 in contact with it.
  • the rod 4e therefore maintains a pool of molten material 2 in its immediate vicinity and near its base (as indicated in Fig. IE) and this pool is surrounded by solid pellets 7.
  • Suitable material for making the conductive rod 4e depends on the composition of the evaporative material 2 to be melted. Generally, material which is suitable for making the melting crucible le is suitable for making the conductive rod 4e. Desirably therefore, the conductive rod 4e is made of material which is substantially inert to the evaporative material 2 at the conditions under which the evaporative material is melted and evaporated. When the evaporative material 2 is silicon, the conductive rod 4e is desirably carbon.
  • the solid pellets 7 can initially be melted either by means of an arc which can be generated by a cathode 35e which is connected via a power supply 26e to the melting crucible le, or by the heater and power supply means already described under Fig. la to Id. Where an arc is to be used this can be achieved by switching the electrode 35e, which is similar to electrode 35 as shown and described with Fig.
  • Electrode 20 as described hereunder with Fig.
  • the rod 4e can take the form of various other electrically conductive elements such as a plate or the like. Also, a plurality of rods 4e may be applied.
  • the electrode system 35e may be used by means of switches 81 and 82 to heat or melt the solid pellets 7 whenever the electrical connection of rod 4e with the base of crucible le becomes inadequate.
  • the heating using electrode 35e is maintained by means of switches 81 and 82 until the current flow through rod 4e restarts due to the electrical conduction of the silicon in the base of crucible le.
  • the electrical current flowing in rod 4e forces some molten material 2 to flow to its rod ends 4'e and 4"e, due to electromagnetic forces whereby 4"e is above level 9e.
  • a thin film of molten material 2 flows up to rod-end 4"e, where it meets the hottest part of rod 4e, because this part must conduct the whole electrical current from power supply 6e in contrast to the parts of rod 4e which are in full contact with electrically-conducting molten material 2, such as in the case of rod-end 4'e, since the molten material 2 helps to augment the circuit.
  • the evaporative material 2 comes in contact with the hottest part of rod 4e (i.e.
  • rod-end 4"e it evaporates and the vapor is emitted from vapor releasing opening 13e.
  • the power supply 6e to rod 4e is adjusted to give the required evaporation rate of material 2 and this maintains a quantity of molten material 2 in contact with rod 4e, which in turn maintains the electrical circuit and enables the evaporation to continue.
  • Fig. 2 illustrates an electric arc discharge apparatus including two identical electrodes 20 comprising a disc 21 of a suitable, coating process specific material to which a DC-potential is connected, an electrical insulating sleeve 22, a hood 23, and a cooling system 24, which comprises water-cooled chambers in good thermal contact with the disc 21.
  • the discs 21 of the electrodes 20 are connected to a switching system 25 which in turn is connected to an adjustable DC-power supply 26 whose energy output is regulated by conventional means.
  • the switching system 25 enables the polarity (+ or -) of the two electrodes to change, so that when one electrode A becomes negatively charged, i.e. cathodic, electrode B simultaneously becomes positively charged, i.e. anodic, and vice- versa.
  • cathodic i.e. negative polarity state
  • a stream of electrons emerges from disc 21 and ionizes the vapor from evaporator system 27 to form a plasma.
  • the discs 21 erode during the electric arc process and the rate of erosion is dependent on the material chosen.
  • the eroded material passes to the gas phase, and is ionized to form a plasma within the space defined by hood 23 and disc 21, it mixes with the plasma formed from the vaporized particles from evaporation system 27. It is often desirable to choose the material of disc 21 such that its erosion particles can form a property-enhancing dopant within the coating.
  • the compositions of the disks 21 of the two electrodes A and B can even be different so as to add multiple components to the coating vapor.
  • a silicon oxide by evaporating silicon (or a silicon oxide) in evaporator system 27 it is often desirable to add dopants to the main coating supplied by evaporator system 27 through the addition of the erosion particles from disc 21.
  • dopants are disclosed in PCT International Application PCT/US 98/05293. and these can either be alloyed within the basic material of disc 21 or disc 21 can be entirely composed of them.
  • Common basic materials for disc 21 are brass and magnesium.
  • the material of the hood 23 should remain essentially inert to the electric arc discharge process and thus resist erosion and corrosion. For example, stainless steel is appropriate for many applications.
  • the electrodes A and B and an evaporator system 27 are disposed in a vacuum cell (such as in Fig. 6) which is capable of maintaining a vacuum.
  • the evaporator system 27 produces a vapor from a solid either by a method as described by Fig. 1, or by any other means, such as the simple means of a conventional, heated crucible.
  • the evaporator system 27 is positioned so that the vapor emerging from the evaporator system mainly passes through the gap between electrodes A and B.
  • Electrodes A and B are oppositely charged, an electrical discharge occurs between them, and a plasma is formed consisting of the ions and electrons discharged from the discs 21, ionized material produced from vapor from evaporator system 27, and ionized reactive gases, if used.
  • Reactive gas or gases are fed into the space between electrodes A and B, when reactive gases are a necessary component of the coating.
  • An example of the use of reactive gas is the application of oxygen as reactive gas with a silicon vapor in a vacuum cell to produce a transparent silicon dioxide coating and is described in U.S. Patent Application Serial No. 08/818,342 filed by Plester et al and PCT International Application PCT/US98/05293, already incorporated by reference.
  • electrodes A and B The detailed operation of electrodes A and B is as follows.
  • electrode A When electrode A is to be the cathode and B is to be the anode, electrode A is switched to the negative polarity by switch 25 and electrode B to positive polarity.
  • An electric discharge arc is formed between the two electrodes and disc 21 of electrode B gradually becomes coated with particles from the evaporator system 27 and disc 21. Meanwhile, disc 21 of electrode A begins to vaporize and erode due to the discharge of particles.
  • the coating of disc 21 of electrode B with particles would lead to the disruption of the arc between the two electrodes if, as in case of silicon dioxide or silicon, the coating particles are electrically non-conducting.
  • the arc intensity, set up between electrodes A and B, and the degree of ionization of the vapor from the evaporator system 27 are regulated by the energy input of the electrode power-supply 26, which is independent of the power supply for the evaporator system.
  • the arc set up between electrodes A and B may die out depending on the rapidity of switching.
  • Each electrode A and B is fitted with an ignition system 28 which conventionally consists of a mechanically operated metal finger or electrically conductive element, which is connected by connection 29 to the anode of the DC power supply, and is made momentarily to touch disc 21 of the cathodic electrode at the instant of ignition, so as to recommence ignition and restart the discharge arc between the electrodes.
  • Connection 29 can inco ⁇ orate an electrical resistor 29a and a switch 29b, as required to control the ignition system.
  • evaporator 27 Although only one evaporator 27 is shown in Fig. 2. it should be understood that the arrangement of electrodes A and B can be used to ionize vapors from a plurality of evaporators producing an ionized gas mixture from a variety of vapors of different composition.
  • Fig. 2a shows an alternative arrangement to that of Fig. 2, which avoids the need for re-ignition when the electrodes 20 in the A and B positions of Fig. 2 switch polarity.
  • two sets of electrodes denoted 20A, 20B and 20C, 20D, are employed and each set has a separate DC-power supply 26 and switching system 25.
  • the switching of the two sets of electrodes is phased so that only one set is switching polarity at any instant, leaving the other set to maintain a plasma.
  • this plasma acts as re-ignition means for the electrodes.
  • FIG. 3 shows an electrode 35 comprising a disc 21, to which the cathodic terminal of a DC-power supply 26 is connected, an electrical insulating sleeve 22 for the disc 21, an anodic hood 23 in the shape of a tapered shell at least partially covering the disc, and a cooling system 24 for cooling the disk 21.
  • the anodic terminal of the adjustable DC power supply 26 is connected via a fixed resistor 36 and a switch 37 to the anodic hood 23.
  • the electrode 35 in Fig. 3 can be constructed identically to electrode 20 in Fig. 2 and the only difference in principle is the connection of the anodic hood 23 to the anodic terminal of power supply 26.
  • Vapor is generated by an evaporator system 27 adjacent the electrode 35 in a vacuum cell (not shown).
  • the function and embodiment of the evaporator system 27 follows the description already given for Fig. 2.
  • the anodic hood 23 has the function of shielding its own interior surface and the cathodic disk 21 from coating vapor emitted by the evaporator 27.
  • a cathodic discharge arc is established in an ionization chamber within the combined anode/cathode electrode 35 between the in-built cathode disc 21 and the integral, anodic hood 23.
  • This discharge is emitted from the hood 23 through a plasma discharge opening 23a into the vapor rising from evaporator system 27, energizing this vapor, and forming a plasma which consists of ionized particles from disc 21, electrons from disc 21 and ionized particles . within the vapor emitted by evaporator system 27.
  • the degree of plasma enhancement can be regulated by the energy input of the power supply 26, which in turn is regulated by conventional means and is independent of the power supply for the evaporator 27.
  • Ignition can be by means of the ignition system 28, as already described under Fig. 2.
  • the discharge from disc 21 forms a plasma which condenses and deposits within the anodic hood 23 when the combined electrode 35 is shut down.
  • This deposit consists of electrically conducting particles, which bridge across the gap between disc 21 and hood 23, causing a short-circuit whenever the electrode 35 ceases to be energized.
  • the energizing switch 37 is closed and energy is reapplied to electrode 35, there is a momentary short-circuit between the cathodic disc 21 and the anodic hood 23 enabling ignition.
  • the short-circuit does not persist because the deposit bridging the cathodic disc 21 with the anodic hood 23 re- evaporates immediately after ignition, and this permits electrode 35 to ignite and commence normal operation.
  • the combined anode/cathode electrodes 35 can be used to ionize vapors from a plurality of evaporators producing a variety of vapors of different composition.
  • the temperature increase in the ionization chamber formed by the disk 21 and the anodic hood 23 can rise to a point where the anodic hood erodes significantly.
  • the erosion of the anodic hood 23 can be reduced or prevented by cooling the outside of the anodic hood, for example, by means of a water jacket 38 and inlet and outlet water flows 39' and 39".
  • Fig. 4 shows an embodiment of an electric arc discharge apparatus, as already described in the case of electrodes 20 and 35, where the erodable component can be continuously replaced and comprises an electrode member 21a in the form of a bar or rod which can be continuously replaced by a plurality of electrode members 21a and which is identical in operating principle to the disc 21 in Figs. 2 and 3.
  • This continuously fed electrode is particularly advantageous when the electrode members 21a are composed of a material which quickly vaporizes during electric arc discharge. Materials for the electrode members 21a which quickly vaporize or " erode are often beneficial because they help energize, ionize, and enhance the plasma.
  • Each electrode member 21a is continuously fed, in series, from a housing 59 defining a loading chamber so that one of the plurality of electrode members is fed to an electric arc discharge position E at a time.
  • the one electrode member being fed is gripped between two water-cooled, semi-circular cold segments 40a and 40b.
  • the cold segments 40a and 40b are served by flexible cooling water pipes 41 , and are mounted on two arms 42a, 42b which are held by a hinge 43 and forced together or apart, when desired, by conventional mechanical means 44 (not shown in detail) which could involve a conventional electrically activated piston, or similar mechanism.
  • the two cold segments 40a, 40b and the two arms 42a, 42b are in electrical contact with the cathodic terminal of a DC power supply 26, as already described.
  • Hinge 43 is connected to a support bracket (not shown), which itself is mounted in an electrically insulated manner.
  • the hood 23, already described in conjunction with Figs. 2 and 3, is split into 2 halves, forming a split-hood 45 and the two halves of split-hood 45 are mounted via electrically insulating mountings on arms 42a, 42b, so that one half of the split-hood 45 is mounted on each arm 42a and 42b and the two halves of the split-hood come together to form a complete hood when the arms 42a, 42b are forced together by mechanical means 44.
  • the split hood 45 is arranged to form an ionization chamber into which the electrode members 21a are fed. For the sake of clarity, split-hood 45 is shown in broken lines in Fig. 4. to avoid over-complicating the presentation.
  • an insulating sleeve 46 which is constructed of an inert, insulating, high temperature tolerant material, such as glass or ceramic, and is supported, along with the housing 59 by a bracket 47.
  • the rearward end of the electrode member 21a being fed to the discharge position E is pressed against a piston 48 which can be moved by a drive means 49.
  • arms 42a, 42b open periodically at fixed time intervals, determined by the process and the rate of erosion of the electrode member, and drive means 49 pushes the electrode member 21a in direction B by an amount which compensates for the erosion. Erosion rates of the electrode member 21a can be accurately determined by proper control of current from power supply 26 and of material purity of the electrode member 21.
  • a magazine 50 holds numerous unused electrode members 21a.
  • Stops 51 hold the stack of unused discs 21 and allow one unused electrode member 21 to enter position C when a positioner 52 on drive means 49 determines that drive means 49 has advanced to a point where position C is clear and therefore can accommodate a replacement electrode member 21a. At that point, stops 51 are opened by activators 53 and allow just one replacement electrode member 21 to drop into position C. Stops 51 and activators 53 together form a conventional feed escapement, and will not be described further.
  • the electrode members 21 a have a protrusion 54 on the rearward end and a matching cavity 55 on the forward end, as marked by direction B, such that the protrusion and cavity fit and grip together when pushed by piston 48.
  • the drive means 49 withdraws in direction D to make space for the replacement electrode member 21a which is then allowed by stops 51 to fall into position C.
  • Drive means 49 then advances to push replacement disc 21 a till the cavity 55 on its front end engages and locks with the protrusion 54 on the rearward end of the particular electrode member 21a which is in actual use at that time in the discharge position E. Thereafter, the drive means 40 continues periodically to advance the electrode member 21a to keep pace with erosion, in the manner already described.
  • the system described by Fig. 4 is intended to be mounted within a high vacuum enclosure and the magazine 50 can be refilled during maintenance shutdowns.
  • the magazine 50 can also be fed from outside the vacuum enclosure by providing an evacuation cell 50a located in communication with the vacuum enclosure and consisting of a separate chamber which can be sealed by two doors 56a, 56b.
  • the separate evacuation cell 50a is brought to atmospheric pressure by closing door 56b and opening door 56a.
  • the evacuation cell 50a is then filled with electrode members 21.
  • Door 56a of the second compartment 50a is then closed and the second compartment 50a evacuated by operating valve 57.
  • door 56b is opened and electrode members 21 are allowed to roll in a controlled manner down a chute from compartment 50a to compartment 50. This procedure can be repeated indefinitely, without the main vacuum enclosure being vented.
  • the system described in Fig. 4, 4A, and 4B can be used as a continuously fed means instead of electrode 20 in Fig. 2, or electrode 35 in Fig. 3, when a continuous feed is required.
  • Fig. 5 shows a means of continuously measuring the rate of evaporation from an evaporator system 27, whether evaporator system 27 is a simple, electrically heated crucible or a continuously fed system as described by Fig. 1 , or a cathodic-arc-heated crucible as in PCT
  • Fig. 5 also shows a means of measuring the degree of ionization within the plasma.
  • the plasma can be generated by an electric arc discharge apparatus such as illustrated in Figs. 2, 3, or 4, or by other means.
  • the plasma making means actually shown is the combined anode/cathode electrode 35 by way of example only.
  • rate of evaporation and degree of ionization these said factors can be regulated, using the measurement data, either automatically or manually.
  • the rate of evaporation can be regulated by the conventionally adjustable energy input of power supply of the evaporator system 27 and the degree of ionization can be regulated by the conventionally adjustable energy input of the power supply 26 of the electrode 35.
  • the measuring device in Fig. 5 includes an electrically conductive element which is a wire 60, supported in an appropriate position within a vacuum vapor deposition coating chamber by an electrically insulated support 61.
  • the electrically conductive element 60 could be another type of conductive member such as a plate or rod.
  • the wire 60 is connected to a power supply 62 via a switch 63. When the switch 63 is closed, the wire 60 is heated, and when the switch 63 is open, the wire 60 cools. The switch 63 is opened/closed by a timer 64 which controls the open/close sequence appropriately.
  • the wire 60 is placed within and exposed to the plasma to be measured and controlled.
  • a DC-power source 65 is connected via an ammeter 66 to the wire 60 and forms a circuit via the ionized particles from source 27 and via the inside of the walls of the vacuum cell 70 to ground, whereby the current generated in this circuit is related to the electrical resistance of the plasma and thus to the degree of ionization.
  • the I/U (current/voltage) diagram shows that the degree of ionization is proportional to the current (I) generated.
  • I current
  • the I/U curve is displaced (see chain-dotted curve in Fig. 5A).
  • the current reverts to being a measure of the degree of ionization (see solid- line curve in Fig. 5A). The fixed time period and the relationship between current and degree of ionization must be determined experimentally for the specific process.
  • the heater circuit 67 is switched off by opening switch 63. This allows coating particles to build up on wire 60 and an evaporation rate measurement can begin.
  • the rate of change of the current measured by ammeter 66 is related to the rate of deposition of non-electrically conducting particles onto wire 60, and this gives a measure of rate of evaporation.
  • Fig. 5b A means of avoiding this disruption of the measurement circuit is shown in Fig. 5b.
  • the measurement circuit now runs from AC or DC power source 65' to wire 60, via the ionized particles to wire 60a and back to power source 65' (the symmetrical use of similarly-sized wires 60a and 60 enables chice of AC or DC power supply).
  • Wire 60a receives coating particles in the same way as the inner walls of the vacuum cell, but remains unaffected because these particles are removed during the heating cycle of wire 60a.
  • FIG. 6 shows a vacuum cell 70 for coating articles by the processes described above, and illustrates, in schematic form, an evaporator source 76, such as illustrated in Fig. 1, or another source of coating vapor, an article to be coated, i.e. coating substrate 77, plasma making electrodes 78 such as those disclosed in Figs. 2-4, and a device 80 for measuring process parameters as illustrated in Fig. 5, all disposed in the vacuum cell.
  • an evaporator source 76 such as illustrated in Fig. 1, or another source of coating vapor
  • an article to be coated i.e. coating substrate 77
  • plasma making electrodes 78 such as those disclosed in Figs. 2-4
  • a device 80 for measuring process parameters as illustrated in Fig. 5 all disposed in the vacuum cell.
  • probes 71 are located within the vacuum enclosure 70, mounted in insulating-sleeves 72 and connected to an ionizing power supply 73.
  • the power supply 73 can be HF, or RF, or DC.
  • Sufficient power must be supplied by the power supply 73 to cause the gas in the vacuum enclosure 70 to ionize.
  • the process of ionizing the gas in enclosure 70 quickly vaporizes deposits within the enclosure 70 and burns these up when they are combustible (as for example, organic deposits due to condensation of vapor emanating from plastic substrates). This reduces the frequency of the need to undertake more time consuming and labor intensive cleaning.
  • This cleaning process using strategically mounted probes 71 throughout the vacuum enclosure 70, can be ignited periodically, normally without interrupting the coating process. Alternatively, it can be applied during brief shut-downs of the coating process, particularly where the cleaning of the inside of vacuum enclosure 70 can be enhanced by increasing pressure, typically in the range from 1 to 10 ⁇ 2 mbar.
  • the material of probes 71 must be suitable for the chosen form of power supply (HF or RF or DC) and resist corrosion under the process conditions in enclosure 70. Examples of suitable materials are stainless steel, copper and titanium.

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Abstract

L'invention concerne des appareils et des procédés à utiliser dans l'enrobage par dépôt sous vide, qui permettent un fonctionnement plus simple, plus économique et continu. Dans un système et un procédé de fusion et d'évaporation continues d'une matière solide pour la formation d'une vapeur d'enrobage, on utilise un creuset de fusion séparé et un creuset d'évaporation. L'invention porte également sur un système et un procédé d'excitation des solides d'évaporation, de sorte qu'un plasma soit formé: Ledit système comporte des première et deuxième électrodes et un dispositif pour changer sélectivement la polarité entre les première et deuxième électrode et empêcher le dépôt de vapeur d'enrobage sur les électrodes. L'invention se rapporte encore à un autre système et procédé pour l'excitation de solides d'évaporation de sorte qu'un plasma soit formé, dans lesquels on utilise un appareil à décharge d'arc électrique, comprenant une partie cathodique et une partie anodique. Une électrode alimentée en continu pour la vaporisation continue des éléments d'électrodes dans une décharge d'arc électrique est décrite. Un appareil et un procédé sont prévus pour la mesure de la vitesse d'évaporation dans un évaporateur et le degré d'ionisation dans un système d'enrobage par dépôt en phase vapeur. Par ailleurs, un système pour le nettoyage in-situ de dépôts vaporisables pour le nettoyage de l'enceinte du système de dépôt sous vide est décrit.
PCT/US1999/015828 1998-08-03 1999-07-14 Systemes d'evaporation sous vide activee par plasma, dont les systemes pour l'evaporation d'un solide, la production d'une decharge d'arc electrique et la mesure de l'ionisation et de l'evaporation Ceased WO2000008226A2 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
AU49906/99A AU4990699A (en) 1998-08-03 1999-07-14 Plasma-enhanced vacuum vapor deposition systems including systems for evaporation of a solid, producing an electric arc discharge and measuring ionization and evaporation
IL14081199A IL140811A0 (en) 1998-08-03 1999-07-14 Plasma-enhanced vacuum vapor deposition systems including systems for evaporation of a solid, producing an electric arc discharge and measuring ionization and evaporation
CA002338352A CA2338352A1 (fr) 1998-08-03 1999-07-14 Systemes d'evaporation sous vide activee par plasma, dont les systemes pour l'evaporation d'un solide, la production d'une decharge d'arc electrique et la mesure de l'ionisation et de l'evaporation
JP2000563847A JP2002522637A (ja) 1998-08-03 1999-07-14 固体の蒸発、アーク放電、及びイオン化と蒸発の測定のための諸システムを含んだプラズマ強化真空蒸着システム
BR9912722-9A BR9912722A (pt) 1998-08-03 1999-07-14 Sistema e processo para fundir e evaporar continuamente um material sólido, sistema de revestimento por deposição de vapor, eletrodo continuamente alimentado, aparelho de descarga de arco elétrico , processos para produzir uma descarga de arco elétrico, para revestir por deposição de vapor, para ionizar um vapor de revestimento, para medir o grau de ionização e a taxa de evaporação a partir de um evaporador em um sistema de revestimento por deposição de vapor e para remover material depositado em uma célula de vácuo por um vapor de revestimento
KR1020017000786A KR20010083127A (ko) 1998-08-03 1999-07-14 고체의 증발용 시스템을 포함하고, 전기 아크 방전을생성하고 및 이온화와 증발을 측정하는 플라즈마 강화진공 증기 증착 시스템
EP99933968A EP1109944A2 (fr) 1998-08-03 1999-07-14 Systemes d'evaporation sous vide activee par plasma, dont les systemes pour l'evaporation d'un solide, la production d'une decharge d'arc electrique et la mesure de l'ionisation et de l'evaporation

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Application Number Priority Date Filing Date Title
US09/128,456 US6251233B1 (en) 1998-08-03 1998-08-03 Plasma-enhanced vacuum vapor deposition system including systems for evaporation of a solid, producing an electric arc discharge and measuring ionization and evaporation
US09/128,456 1998-08-03

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WO2000008226A2 true WO2000008226A2 (fr) 2000-02-17
WO2000008226A3 WO2000008226A3 (fr) 2000-12-07

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10024827B4 (de) * 1999-11-17 2008-03-27 Applied Materials Gmbh & Co. Kg Elektrodenanordnung und ihre Verwendung
WO2010095011A1 (fr) 2009-02-18 2010-08-26 Council Of Scientific & Industrial Research Procédé pour déposer du carbone de type diamant sous la forme d'un revêtement protecteur sur une surface interne d'un objet façonné
TWI477625B (zh) * 2012-12-26 2015-03-21 Au Optronics Corp 蒸鍍裝置

Families Citing this family (50)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6223683B1 (en) * 1997-03-14 2001-05-01 The Coca-Cola Company Hollow plastic containers with an external very thin coating of low permeability to gases and vapors through plasma-assisted deposition of inorganic substances and method and system for making the coating
TW490714B (en) 1999-12-27 2002-06-11 Semiconductor Energy Lab Film formation apparatus and method for forming a film
US20020011205A1 (en) 2000-05-02 2002-01-31 Shunpei Yamazaki Film-forming apparatus, method of cleaning the same, and method of manufacturing a light-emitting device
US7517551B2 (en) * 2000-05-12 2009-04-14 Semiconductor Energy Laboratory Co., Ltd. Method of manufacturing a light-emitting device
US6599584B2 (en) * 2001-04-27 2003-07-29 The Coca-Cola Company Barrier coated plastic containers and coating methods therefor
DE10130666A1 (de) * 2001-06-28 2003-01-23 Applied Films Gmbh & Co Kg Softcoat
SG113448A1 (en) * 2002-02-25 2005-08-29 Semiconductor Energy Lab Fabrication system and a fabrication method of a light emitting device
JP2005522572A (ja) * 2002-04-15 2005-07-28 ザ・コカ−コーラ・カンパニー エポキシド添加剤を含有する被膜用組成物及びそれを被覆した構造体
EP1369499A3 (fr) 2002-04-15 2004-10-20 Semiconductor Energy Laboratory Co., Ltd. Méthode et appareillage pour fabriquer un dispositif émetteur de lumière
TWI336905B (en) * 2002-05-17 2011-02-01 Semiconductor Energy Lab Evaporation method, evaporation device and method of fabricating light emitting device
US20040035360A1 (en) 2002-05-17 2004-02-26 Semiconductor Energy Laboratory Co., Ltd. Manufacturing apparatus
KR100838065B1 (ko) 2002-05-31 2008-06-16 삼성에스디아이 주식회사 박막증착기용 고정장치와 이를 이용한 고정방법
US20030221620A1 (en) * 2002-06-03 2003-12-04 Semiconductor Energy Laboratory Co., Ltd. Vapor deposition device
US7601225B2 (en) * 2002-06-17 2009-10-13 Asm International N.V. System for controlling the sublimation of reactants
EP1382713B1 (fr) * 2002-07-19 2006-05-17 Lg Electronics Inc. Source pour dépôt thermique physique en phase vapeur de couches organiques électroluminescentes
US20040123804A1 (en) 2002-09-20 2004-07-01 Semiconductor Energy Laboratory Co., Ltd. Fabrication system and manufacturing method of light emitting device
DE10354625A1 (de) * 2003-11-22 2005-06-30 Sig Technology Ltd. Verfahren zur Bestimmung der Gasdurchlässigkeit von Behälterwandungen, Behälter mit Oberflächenbeschichtung sowie Beschichtungseinrichtung mit Messvorrichtung
US7513953B1 (en) 2003-11-25 2009-04-07 Nano Scale Surface Systems, Inc. Continuous system for depositing films onto plastic bottles and method
US7232588B2 (en) * 2004-02-23 2007-06-19 Eastman Kodak Company Device and method for vaporizing temperature sensitive materials
US20050244580A1 (en) * 2004-04-30 2005-11-03 Eastman Kodak Company Deposition apparatus for temperature sensitive materials
JP4668561B2 (ja) * 2004-07-30 2011-04-13 株式会社アルバック 成膜材料供給装置
DE102005049906B4 (de) * 2005-10-17 2009-12-03 Von Ardenne Anlagentechnik Gmbh Verfahren und Vorrichtung zur Verdampfung von Verdampfungsmaterial
US8261690B2 (en) * 2006-07-14 2012-09-11 Georgia Tech Research Corporation In-situ flux measurement devices, methods, and systems
US8133367B1 (en) * 2006-08-11 2012-03-13 Raytheon Company Sputtering system and method using a loose granular sputtering target
AT503646B1 (de) * 2006-09-15 2007-12-15 Fronius Int Gmbh Wasserdampfplasmabrenner und verfahren zur verschleisserkennung und prozessregelung bei einem solchen wasserdampfplasmabrenner
EP1967606A1 (fr) * 2007-03-08 2008-09-10 Applied Materials, Inc. Creuset d'évaporation et appareil d'évaporation à propriété d'évaporation adaptée
US8061353B2 (en) 2007-03-09 2011-11-22 Global Medical Holdings LLC Method and apparatus for delivering a dose of a gaseous drug to a patient
EP1972699A1 (fr) * 2007-03-20 2008-09-24 ArcelorMittal France Procede de revetement d'un substrat et installation de depot sous vide d'alliage metallique
CN101641457B (zh) * 2007-03-26 2012-04-25 株式会社爱发科 蒸镀源、蒸镀装置、成膜方法
EP2025773A1 (fr) * 2007-07-19 2009-02-18 Applied Materials, Inc. Appareil d'évaporation sous vide pour matériaux solides
US7883745B2 (en) 2007-07-30 2011-02-08 Micron Technology, Inc. Chemical vaporizer for material deposition systems and associated methods
DE102008026001B4 (de) * 2007-09-04 2012-02-16 Von Ardenne Anlagentechnik Gmbh Verfahren und Vorrichtung zur Erzeugung und Bearbeitung von Schichten auf Substraten unter definierter Prozessatmosphäre und Heizelement
JP5228437B2 (ja) * 2007-10-19 2013-07-03 東京エレクトロン株式会社 処理装置及びその使用方法
US20090317547A1 (en) * 2008-06-18 2009-12-24 Honeywell International Inc. Chemical vapor deposition systems and methods for coating a substrate
US8343583B2 (en) * 2008-07-10 2013-01-01 Asm International N.V. Method for vaporizing non-gaseous precursor in a fluidized bed
JP2010144221A (ja) * 2008-12-18 2010-07-01 Tokyo Electron Ltd 原料ガス発生装置及び成膜装置
KR100936378B1 (ko) * 2009-04-27 2010-01-13 에스엔유 프리시젼 주식회사 원료 공급 유닛과 박막 증착 장치 및 박막 증착 방법
EP2369033A1 (fr) * 2010-03-26 2011-09-28 Saint-Gobain Glass France Procédé de remplissage d'une chambre d'évaporateur
US9443703B2 (en) 2011-12-19 2016-09-13 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Apparatus for generating a hollow cathode arc discharge plasma
US9527107B2 (en) * 2013-01-11 2016-12-27 International Business Machines Corporation Method and apparatus to apply material to a surface
JP2014136827A (ja) * 2013-01-18 2014-07-28 Hitachi High-Technologies Corp 蒸着装置およびこれに用いる蒸発源
KR101432514B1 (ko) * 2013-01-29 2014-08-21 한국기초과학지원연구원 플라즈마 보조 물리 기상 증착원
CN105829573B (zh) * 2013-12-19 2018-08-24 Posco公司 加热装置及包括该装置的涂覆机
CN107109626B (zh) * 2014-09-18 2020-07-28 蒂森克虏伯钢铁欧洲股份公司 用于在部件的表面上形成涂层的装置
CN106119781B (zh) * 2016-07-27 2018-10-30 京东方科技集团股份有限公司 蒸发装置、蒸镀设备和蒸镀方法
WO2018020296A1 (fr) 2016-07-27 2018-02-01 Arcelormittal Appareil et procédé de dépôt par évaporation sous vide
US10801101B2 (en) * 2017-08-17 2020-10-13 Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. Vapor evaporation source
TWI634221B (zh) * 2017-09-01 2018-09-01 行政院原子能委員會核能硏究所 電化學元件之製造方法
CN107881485B (zh) * 2017-11-01 2019-10-01 深圳市华星光电半导体显示技术有限公司 等离子体增强化学气相沉积设备及oled面板的封装方法
GB2574400B (en) 2018-06-04 2022-11-23 Dyson Technology Ltd A Device

Family Cites Families (79)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2664852A (en) 1950-04-27 1954-01-05 Nat Res Corp Vapor coating apparatus
US2665226A (en) 1950-04-27 1954-01-05 Nat Res Corp Method and apparatus for vapor coating
US3016873A (en) 1959-01-26 1962-01-16 Nat Res Corp Coating
US2996037A (en) 1959-01-26 1961-08-15 Nat Res Corp Vacuum coating apparatus
US3511703A (en) 1963-09-20 1970-05-12 Motorola Inc Method for depositing mixed oxide films containing aluminum oxide
GB1103211A (en) 1965-01-08 1968-02-14 Mullard Ltd Improvements in and relating to vapour deposition and evaporation sources
US3625848A (en) * 1968-12-26 1971-12-07 Alvin A Snaper Arc deposition process and apparatus
US4024399A (en) * 1975-01-06 1977-05-17 Jersey Nuclear-Avco Isotopes, Inc. Method and apparatus for measuring vapor flow in isotope separation
JPS543853A (en) 1977-06-13 1979-01-12 Onoda Cement Co Ltd Removing device of excess powder for electrostatidc powder coating
JPS5779621A (en) 1980-11-05 1982-05-18 Mitsubishi Electric Corp Plasma processing device
CH645137A5 (de) 1981-03-13 1984-09-14 Balzers Hochvakuum Verfahren und vorrichtung zum verdampfen von material unter vakuum.
JPS57169088A (en) 1981-04-09 1982-10-18 Olympus Optical Co Ltd Crucible
US4532196A (en) 1982-01-25 1985-07-30 Stanley Electric Co., Ltd. Amorphous silicon photoreceptor with nitrogen and boron
DE3239131A1 (de) 1982-10-22 1984-04-26 Ulrich 8950 Kaufbeuren Goetz Verfahren zur thermischen verdampfung von metallen im vakuum
JPS59128281A (ja) 1982-12-29 1984-07-24 信越化学工業株式会社 炭化けい素被覆物の製造方法
GB2139647B (en) 1983-02-24 1986-11-19 Boc Group Plc Bottle coated ion-plating or magnetron sputtering
US4573429A (en) 1983-06-03 1986-03-04 Nordson Corporation Process for coating substrates with aqueous polymer dispersions
US4552791A (en) 1983-12-09 1985-11-12 Cosden Technology, Inc. Plastic container with decreased gas permeability
DE3413891C2 (de) 1984-04-12 1987-01-08 Horst Dipl.-Phys. Dr. 4270 Dorsten Ehrich Verfahren und Vorrichtung zur Materialverdampfung in einem Vakuumbehälter
US5096558A (en) 1984-04-12 1992-03-17 Plasco Dr. Ehrich Plasma - Coating Gmbh Method and apparatus for evaporating material in vacuum
US4634605A (en) 1984-05-23 1987-01-06 Wiesmann Harold J Method for the indirect deposition of amorphous silicon and polycrystalline silicone and alloys thereof
US4615916A (en) 1984-06-25 1986-10-07 Owens-Illinois, Inc. Surface treatment of glass containers
JPS61104075A (ja) 1984-10-23 1986-05-22 Hironobu Sato イオン化蒸発速度制御装置
US4752426A (en) 1985-06-27 1988-06-21 Yoshito Ikada Process for manufacture of plastic resinous tubes
US4697974A (en) 1986-01-24 1987-10-06 Trimedia Corporation Pallet-loading system
DE3623970A1 (de) 1986-07-16 1988-01-28 Leybold Heraeus Gmbh & Co Kg Transporteinrichtung mit rollensystemen fuer vakuum-beschichtungsanlagen
US4902531A (en) 1986-10-30 1990-02-20 Nihon Shinku Gijutsu Kabushiki Kaisha Vacuum processing method and apparatus
US5215640A (en) 1987-02-03 1993-06-01 Balzers Ag Method and arrangement for stabilizing an arc between an anode and a cathode particularly for vacuum coating devices
EP0285745B1 (fr) 1987-03-06 1993-05-26 Balzers Aktiengesellschaft Procédé et dispositifs de déposition sous vide utilisant une décharge électrique
NL8700620A (nl) 1987-03-16 1988-10-17 Hauzer Holding Kathode boogverdampingsinrichting alsmede werkwijze voor het bedrijven daarvan.
JPS63243264A (ja) 1987-03-31 1988-10-11 Matsushita Electric Ind Co Ltd 薄膜製造装置
JPS63312968A (ja) 1987-06-15 1988-12-21 Hitachi Ltd 溶解蒸発装置
US4888199A (en) 1987-07-15 1989-12-19 The Boc Group, Inc. Plasma thin film deposition process
DE3731444A1 (de) 1987-09-18 1989-03-30 Leybold Ag Vorrichtung zum beschichten von substraten
JPH01268859A (ja) 1988-04-20 1989-10-26 Casio Comput Co Ltd 透明導電膜の形成方法および形成装置
JPH02118064A (ja) 1988-10-27 1990-05-02 Mitsubishi Heavy Ind Ltd 真空蒸着装置
JPH02305963A (ja) * 1989-05-19 1990-12-19 Osaka Shinku Kiki Seisakusho:Kk イオンプレーティング装置に於ける材料蒸発速度検出装置及び材料蒸発速度制御装置
DD286375A5 (de) 1989-08-04 1991-01-24 ��@���������@�������k�� Bogenentladungsverdampfer mit mehreren verdampfertiegeln
JP2726118B2 (ja) 1989-09-26 1998-03-11 キヤノン株式会社 堆積膜形成法
JPH07110991B2 (ja) 1989-10-02 1995-11-29 株式会社日立製作所 プラズマ処理装置およびプラズマ処理方法
JPH0733576B2 (ja) * 1989-11-29 1995-04-12 株式会社日立製作所 スパツタ装置、及びターゲツト交換装置、並びにその交換方法
DE4006457C2 (de) 1990-03-01 1993-09-30 Balzers Hochvakuum Verfahren zum Verdampfen von Material in einer Vakuumaufdampfanlage sowie Anlage derselben
US5112644A (en) 1990-03-08 1992-05-12 Optical Coating Laboratory, Inc. Horizontal precession tooling and method for tube rotation
CA2040638A1 (fr) 1990-04-20 1991-10-21 Gedeon I. Deak Materiaux barriere pour emballage
US5084356A (en) 1990-04-20 1992-01-28 E. I. Du Pont De Nemours And Company Film coated with glass barrier layer with metal dopant
US5085904A (en) 1990-04-20 1992-02-04 E. I. Du Pont De Nemours And Company Barrier materials useful for packaging
DE4114108C1 (fr) 1991-04-30 1991-12-19 Schott Glaswerke, 6500 Mainz, De
DE4026494A1 (de) 1990-08-22 1992-02-27 Ehrich Plasma Coating Vorrichtung zur materialverdampfung mittels vakuumlichtbogenentladung und verfahren
DE4100541C1 (fr) 1991-01-10 1992-01-16 Plasco Dr. Ehrich Plasma-Coating Gmbh, 6501 Heidesheim, De
EP0510340B1 (fr) 1991-04-23 1995-05-10 Balzers Aktiengesellschaft Procédé pour retirer du matériau d'une surface dans une chambre à vide
EP0535810B1 (fr) 1991-10-03 1996-03-06 Becton, Dickinson and Company Tube pour le prélèvement du sang
EP0550039B1 (fr) 1991-12-26 1998-03-18 Toyo Boseki Kabushiki Kaisha Film formant barrière aux gaz
DE4200429A1 (de) 1992-01-10 1993-07-15 Ehrich Plasma Coating Verfahren zur ionisation thermisch erzeugter materialdaempfe und vorrichtung zur durchfuehrung des verfahrens
GB2263472B (en) 1992-01-14 1995-09-06 Stalplex Limited Handling and processing plastics bottles
DE4203371C1 (fr) 1992-02-06 1993-02-25 Multi-Arc Oberflaechentechnik Gmbh, 5060 Bergisch Gladbach, De
CH689767A5 (de) * 1992-03-24 1999-10-15 Balzers Hochvakuum Verfahren zur Werkstueckbehandlung in einer Vakuumatmosphaere und Vakuumbehandlungsanlage.
MX9303141A (es) 1992-05-28 1994-04-29 Polar Materials Inc Metodos y aparatos para depositar recubrimientos de barrera.
US5308649A (en) 1992-06-26 1994-05-03 Polar Materials, Inc. Methods for externally treating a container with application of internal bias gas
US5462779A (en) 1992-10-02 1995-10-31 Consorzio Ce.Te.V. Centro Tecnologie Del Vuoto Thin film multilayer structure as permeation barrier on plastic film
US5670224A (en) 1992-11-13 1997-09-23 Energy Conversion Devices, Inc. Modified silicon oxide barrier coatings produced by microwave CVD deposition on polymeric substrates
DE4305721C1 (de) * 1993-02-25 1994-07-21 Dresden Vakuumtech Gmbh Niedervoltbogenverdampfer mit Nachfütterungseinrichtung und Verfahren zu dessen Verwendung
US5677010A (en) 1993-06-01 1997-10-14 Kautex Werke Reinold Hagen Aktiengesellschaft Method for producing a polymer coating inside hollow plastic articles
JPH0794421A (ja) 1993-09-21 1995-04-07 Anelva Corp アモルファスシリコン薄膜の製造方法
US5364666A (en) 1993-09-23 1994-11-15 Becton, Dickinson And Company Process for barrier coating of plastic objects
DE4343042C1 (de) * 1993-12-16 1995-03-09 Fraunhofer Ges Forschung Verfahren und Einrichtung zum plasmaaktivierten Bedampfen
CH687601A5 (de) 1994-02-04 1997-01-15 Tetra Pak Suisse Sa Verfahren zur Herstellung von im Innern sterilen Verpackungen mit hervorragenden Sperreigenschaften.
US5565248A (en) 1994-02-09 1996-10-15 The Coca-Cola Company Method and apparatus for coating hollow containers through plasma-assisted deposition of an inorganic substance
DE4412906C1 (de) * 1994-04-14 1995-07-13 Fraunhofer Ges Forschung Verfahren und Einrichtung für die ionengestützte Vakuumbeschichtung
US5521351A (en) 1994-08-30 1996-05-28 Wisconsin Alumni Research Foundation Method and apparatus for plasma surface treatment of the interior of hollow forms
US5510155A (en) 1994-09-06 1996-04-23 Becton, Dickinson And Company Method to reduce gas transmission
JPH0892764A (ja) 1994-09-22 1996-04-09 Nec Kyushu Ltd スパッタ装置
DE4444763C2 (de) 1994-12-19 1996-11-21 Apvv Angewandte Plasma Vakuum Elektrode zur Materialverdampfung für die Beschichtung von Substraten
DE19600993A1 (de) 1995-01-13 1996-08-08 Technics Plasma Gmbh Vorrichtung und Verfahren zur anodischen Verdampfung eines Materials mittels einer Vakuumlichtbogenentladung
DE19546827C2 (de) 1995-12-15 1999-03-25 Fraunhofer Ges Forschung Einrichtung zur Erzeugung dichter Plasmen in Vakuumprozessen
US5558720A (en) 1996-01-11 1996-09-24 Thermacore, Inc. Rapid response vapor source
EP0785291A1 (fr) 1996-01-19 1997-07-23 The Boc Group, Inc. Système d'évaporation à faisceau d'électrons
US5691007A (en) 1996-09-30 1997-11-25 Becton Dickinson And Company Process for depositing barrier film on three-dimensional articles
US6223683B1 (en) 1997-03-14 2001-05-01 The Coca-Cola Company Hollow plastic containers with an external very thin coating of low permeability to gases and vapors through plasma-assisted deposition of inorganic substances and method and system for making the coating
DE19807032A1 (de) 1998-02-19 1999-08-26 Leybold Systems Gmbh Verfahren und Vorrichtung zum Transportieren zu beschichtender zylindrischer Substrate

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10024827B4 (de) * 1999-11-17 2008-03-27 Applied Materials Gmbh & Co. Kg Elektrodenanordnung und ihre Verwendung
WO2010095011A1 (fr) 2009-02-18 2010-08-26 Council Of Scientific & Industrial Research Procédé pour déposer du carbone de type diamant sous la forme d'un revêtement protecteur sur une surface interne d'un objet façonné
EP2589680A1 (fr) 2009-02-18 2013-05-08 Council of Scientific & Industrial Research Dispositif pour déposer du carbone de type diamant comme revêtement protecteur sur une surface interne d'un objet façonné
TWI477625B (zh) * 2012-12-26 2015-03-21 Au Optronics Corp 蒸鍍裝置

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US6447837B2 (en) 2002-09-10
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US20010022272A1 (en) 2001-09-20
US6251233B1 (en) 2001-06-26
AR025066A2 (es) 2002-11-06
BR9912722A (pt) 2001-05-02
CO5111049A1 (es) 2001-12-26
AR025065A2 (es) 2002-11-06
US20030007786A1 (en) 2003-01-09
CA2338352A1 (fr) 2000-02-17
AR025067A2 (es) 2002-11-06
CN1348509A (zh) 2002-05-08
AR016735A1 (es) 2001-07-25
KR20010083127A (ko) 2001-08-31
AR025064A2 (es) 2002-11-06
CO5111064A1 (es) 2001-12-26
IL140811A0 (en) 2002-02-10
WO2000008226A3 (fr) 2000-12-07
EP1109944A2 (fr) 2001-06-27

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